CN102295306A - Carbonizer for continuously synthesizing calcium carbonate and production method of calcium carbonate - Google Patents
Carbonizer for continuously synthesizing calcium carbonate and production method of calcium carbonate Download PDFInfo
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- CN102295306A CN102295306A CN201110159221XA CN201110159221A CN102295306A CN 102295306 A CN102295306 A CN 102295306A CN 201110159221X A CN201110159221X A CN 201110159221XA CN 201110159221 A CN201110159221 A CN 201110159221A CN 102295306 A CN102295306 A CN 102295306A
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Abstract
The invention relates to a carbonizer for continuously synthesizing calcium carbonate and a production method of calcium carbonate, an input port of calcium hydroxide, an input port of carbon dioxide are provided on the body of the carbonizer, a discharge port is provided at the bottom of the carbonizer, the input port of calcium hydroxide and the input port of carbon dioxide are positioned at the top of the carbonizer body, the transverse trays with displacement from each other are uniformly arranged from the lower part to the bottom of two input ports in the body of the carbonizer, a layout of a S shape backflow baffle plate or a snaky shape backflow baffle plate is used between the adjacent trays. The calcium hydroxide slurry is a fluid suspension, and enables an equidirectional flow with carbon dioxide on the transverse trays between the trays, the calcium hydroxide slurry enters to the next tray from an outlet, three phases of gas, liquid and solid phase are reacted to generate precipitated calcium carbonate, the reacted material-carbonized boiled slurry is flowed out from the outlet of lower part of the reactor. The product has the advantages of adjustable particle size, narrow grain size distribution and stable quality, dispersibility, stability and alkali efflorescence are improved; the invention has the advantages of less equipment investment, short reaction time, less energy consumption, low cost, and the product enables continuous production.
Description
Technical field
The present invention relates to a kind of method and equipment thereof of continuous synthetic calcium carbonate, be meant the synthetic method of lime carbonate and the used carbonization reactor thereof produced of a kind of continuous carbonization especially.
Background technology
Precipitated chalk is important inorganic powder material, and at present both at home and abroad the industrialized producing technology of precipitated chalk mainly contains: intermittently bubbling carbonizing method, spray multistage carborization, continuous bubbling carbonizing, high-gravity reactive precipitation, the tower carborization of vertical sieve tray, internal circulating carbonator preparation method continuously.Bubbling carbonizing method at intermittence wherein, continuous bubbling carbonizing are generally adopted to prepare subparticle lime carbonate, and it is to contain CO
2Gas feed Ca (OH) be housed
2Slurries with or without finishing carburizing reagent in the bubble tower of agitator or the retort, by the refrigeration control reaction temperature with add the preparation that additives such as dispersion agent, crystal formation control agent are realized fine calcium carbonates.Because the ununiformity that gas phase distributes, cause the alternate interface contact area of gas, liquid, solid three little.Prepare subparticle lime carbonate with this synthetic method and equipment and have following problem and shortage: the product particle particle size distribution range that (1) produces is wide; (2) the median size fluctuation range is big between different batches; (3) being easy to generate the parcel phenomenon in the reaction process finally causes the product accumulation of salt in the surface soil to influence quality product; (4) these two processes of nucleation and crystal growth are not separated, and wish to get the solid phase particles of big or small uniformity, the difficult control of processing condition; (5) production process needs lower temperature operation (generally being lower than 25 ℃), and energy consumption is higher; (6) the carburizing reagent time long, batch production energy consumption height yields poorly CO
2Utilization ratio is low.
Summary of the invention
The purpose of this invention is to provide a kind of continuous production, grade narrowly distributing, dispersiveness, stability and the accumulation of salt in the surface soil all improves, constant product quality, low equipment investment, carburizing reagent time are short, power consumption less, cost is low, but the continuous production particle diameter is less than the nano-calcium carbonate calcium product of 100 nanometers and particle diameter carbonation reaction tower and the production method thereof greater than the fine calcium carbonate product and the micron-sized common light calcium carbonate product of 100 nanometers.
Designed a kind of carbonizer of continuous synthetic calcium carbonate according to above-mentioned purpose, comprised this carbonizer jar shape body, described body is provided with calcium hydroxide Ca (OH)
2Slurries input aperture, carbonic acid gas CO
2The input aperture is provided with discharge port, described Ca (OH) in this body bottom
2Slurries input aperture and CO
2The input aperture all is positioned at the top of body, is provided with the horizontal column plate of outlet mutual dislocation below these two input apertures of body interior equably to the bottom.Be provided with and the perpendicular sieve plate of the first layer column plate in the exit of described the first layer column plate; Described CO
2The input aperture is array architecture in body so that CO
2Be covered with equably in the cavity volume of body, and what adopt between the outlet of described adjacent tray is S shape or snakelike reverse-flow baffle layout.
Utilize the method steps of the carbonizer production lime carbonate of aforesaid continuous synthetic calcium carbonate to be:
(1) calcining step--calcined limestone gets unslaked lime;
(2) the unslaked lime maturation stage--unslaked lime is converted water cure, system lime white refining liquid;
(3) carburising step--the lime extract slurries are pumped into carbonization reactor carry out carburizing reagent production precipitated chalk particle, and obtain to contain the ripe slurry of precipitated chalk particle;
(4) processed--to getting filter cake after the ripe slurry dehydration after the activation;
(5) drying treatment--filter cake is carried out drying and metering packing; Wherein,
Described carburising step is:
A. refining liquid is sent into Ca (OH)
2Slurry tank, and with deployed Ca (OH)
2Refining liquid is sent into the reactor bubble level from reactor top, simultaneously carbon dioxide is imported carbonization reactor;
Described Ca (OH)
2Refining liquid is suspension, on the horizontal column plate of this suspension in reactor and carbonic acid gas equidirectional flow between column plate, flow to the outlet that is positioned at the other end by an end, suspension enters down one deck column plate from outlet, carry out the gas, liquid, solid phase reaction in the flow process and generate precipitated chalk, reacted material is that the good ripe slurries of carbonization flow out from the reactor lower part outlet;
B. collect from reactor behind the effusive material this material carried out ageing and recarbonize or directly activate after, more after filtration, be drying to obtain product.
The present invention is directed to the problem and shortage that " bubbling carbonizing method " preparation subparticle lime carbonate exists, provide a kind of and can make that product cut size is adjustable, the grade narrowly distributing; Dispersiveness, stability and the accumulation of salt in the surface soil all improve, constant product quality, low equipment investment, carburizing reagent time are short, power consumption less, cost is low, but the continuous production particle diameter less than the nano-calcium carbonate calcium product of 100 nanometers and particle diameter greater than the fine calcium carbonate product of 100 nanometers and the new process and the carbonization reactor of micron-sized common light calcium carbonate product.Compared with prior art, the present invention adopts column plate type carbonization reactor continuous production calcium carbonate product, and is with the obvious advantage, is embodied in:
But 1 continuous production;
2, because of separating in carbonization crystal nucleation phase and vegetative period, the nucleation reaction period is positioned at reactor upper tray zone or bubbling zone, is arranged in reactor, lower region vegetative period, and the nucleation areal pressure is big than the growth district reaction pressure, temperature is low, CO
2Gas and Ca (OH)
2The concentration height, the lime carbonate degree of supersaturation height that generates, become nuclear volume big, flow out the nucleation district after the nucleation and enter the vitellarium, compare with the gap bubbling carbonizing, particle is short in the residence time in nucleation period, the titanium pillaring solution that nucleation period generates time on the nucleus that generates is short and consistent, and the calcium carbonate product particle diameter that is generated is little, and crystalline form is regular, particle size distribution range is narrow, constant product quality;
3, adopt the column plate carbonization synthetic, gas, liquid, solid phase reaction contact surface is big, the degree of supersaturation height, and carbonization time is short, CO
2The utilization ratio height, output height, but continuous production, energy consumption is low, and facility investment and maintenance cost significantly reduce;
4, process adjustments is easy and simple to handle, and the whole process continuous production is by reaction pressure, temperature, CO
2Gas and Ca (OH)
2The adjusting of concentration height and flow can make things convenient for and regulate neatly the particle diameter of precipitated chalk product, easily is automated production control, can realize that online computer controls automatically, is beneficial to the large-scale industrial production precipitated chalk.
Description of drawings
Accompanying drawing 1 is the main TV structure simplified schematic diagram of carbonizer among the present invention; Accompanying drawing 2 is schematic flow sheets of producing lime carbonate in the inventive method.
Embodiment
Purport of the present invention is the improvement by carbonizer, makes the production realization serialization of lime carbonate, controlledization of lime carbonate grain size.
With reference to accompanying drawing, basic design scheme disclosed by the invention is:
A kind of carbonizer of continuous synthetic calcium carbonate comprises this carbonizer jar shape body 1, and described body is provided with calcium hydroxide Ca (OH)
2Slurries input aperture 2, carbonic acid gas CO
2Input aperture 3 is provided with discharge port 4, described Ca (OH) in this body bottom
2Slurries input aperture and CO
2The input aperture all is positioned at the top of body, below these two input apertures of body interior, be provided with equably to the bottom outlet 6 mutual dislocation horizontal column plate 5 and, what adopt between the outlet of adjacent tray is S shape or snakelike reverse-flow baffle layout.Outlet 52 places at described the first layer column plate 51 are provided with the sieve plate 53 perpendicular with the first layer column plate; Described CO
2The input aperture is array architecture in body so that CO
2Be covered with equably in the cavity volume of body.
Utilize the step of the carbonizer production lime carbonate method of the continuous synthetic calcium carbonate of the present invention to be:
(1) the quicklime slaking operation that obtains behind calcining step--Wingdale and the coal calcination, CO
2Gas is carbon elimination CO after purifying treatment
2The gas buffer jar.
(2) unslaked lime maturation stage--unslaked lime and water is by lime: water=1: 3～7 (weight ratio) carries out slaking, and the refining liquid after sieving is mixed with and contains Ca (OH)
2The refining liquid of mass concentration 5%～15% enters Ca (OH) after transferring to technological temperature
2Slurry tank.
(3) carburising step--with deployed Ca (OH)
2Refining liquid is sent into the reactor bubble level by reactor top, and the calcium hydroxide suspension concentration that enters reactor is 5%～15%, and temperature is 10 ℃～60 ℃; The carbon dioxide that passes through water washing cleaning simultaneously enters carbonization reactor bubble level (being the first layer) by flowrate control valve and carries out the bubbling carbonizing reaction, enter carbon dioxide volumetric concentration 〉=15% of reactor, absolute pressure is 0.1MPa～1.0MPa, and refining liquid (being material) carries out Ca (OH) on the multilayer column plate in reactor
2+ CO
2=CaCO
3+ H
2The carbonization building-up reactions of O, Ca (OH)
2On the horizontal column plate of suspension in reactor and CO2 gas equidirectional flow between column plate, after flowing to the other end by an end opening is arranged, material in reaction back and the reaction enters down one deck column plate from opening, carry out the gas, liquid, solid phase reaction in the flow process and generate precipitated chalk, material flows out continuously from reactor lower part and enters dehydration procedure behind the reaction terminating.
The lime extract slurries are pumped into carbonization reactor carry out carburizing reagent production precipitated chalk particle, and obtain to contain the ripe slurry of precipitated chalk particle;
(4) processed--the ripe slurry after the activation is squeezed into plate-and-frame filter press by ripe stock pump and is dewatered, and filter cake is sent to drying process;
(5) drying treatment--filter cake is carried out drying and metering packing.
The invention will be further described below in conjunction with accompanying drawing.
Embodiment 1
Shown in Figure 2 as process flow diagram, to CO
2It is that 28% the limestone kiln kiln gas after purifying is CO that surge tank feeds volumetric concentration
2(down together) is toward Ca (OH)
2Slurry tank is squeezed into allotment back its Ca (OH)
2Concentration is 8%, temperature is 25 ℃～26 ℃ Ca (OH)
2Slurries are opened and are stirred adding weight ratio 0.2%Ca (OH)
2The meter citric acid; Feeding gauge pressure with 18 cubic meters per minute flows to carbonization reactor earlier is the 0.2MPa kiln gas, pumps into Ca (OH) with 20 cubic metres of/hour flows to carbonization reactor then
2Slurries, the Ca that pumps into (OH)
2Slurries are moving at bubbling carbonizing laminar flow as shown in Figure 2, in the flow process with the kiln gas generation carburizing reagent of sending by the kiln gas distribution piping, overflow to down one deck column plate from sieve plate or sieve plate top after flowing to the other end, continue and kiln gas generation carburizing reagent from sieve plate top equidirectional inflow column plate layer, go out from the carbonation reaction tower tower bottom flow at last, obtaining pH value in the carbonation reaction tower outlet is 7～8, and particle diameter is the calcium carbonate serosity of 50 nanometers, narrowly distributing, good dispersity.
Embodiment 2
To CO
2Surge tank feeding volumetric concentration is 28% the limestone kiln kiln gas after purifying, toward Ca (OH)
2Slurry tank is squeezed into Ca (OH)
2Concentration is 8%, temperature is 30 ℃～31 ℃ Ca (OH)
2Slurries are opened and are stirred adding weight ratio 0.5%Ca (OH)
2Meter sal epsom; Feeding gauge pressure with flow 36 cubic meters per minute to carbonization reactor earlier is the 0.15MPa kiln gas, pumps into Ca (OH) with 30 cubic metres of/hour flows to carbonization reactor then
2Slurries, the Ca that pumps into (OH)
2Slurries are moving at illustrated bubbling carbonizing laminar flow, in the flow process with the kiln gas generation carburizing reagent of sending by the kiln gas distribution piping, overflow to down one deck column plate from sieve plate or sieve plate top after flowing to the other end, continue and kiln gas generation carburizing reagent from sieve plate top equidirectional inflow column plate layer, go out from the carbonation reaction tower tower bottom flow at last, obtaining pH value in the carbonation reaction tower outlet is 7～8, and particle diameter is the calcium carbonate serosity of 200 nanometers, narrowly distributing, good dispersity.
Embodiment 3
To CO
2Surge tank feeding volumetric concentration is 28% the limestone kiln kiln gas after purifying, toward Ca (OH)
2Slurry tank is squeezed into Ca (OH)
2Concentration is 8%, temperature is 40 ℃～45 ℃ Ca (OH)
2Slurries; Feeding gauge pressure with flow 52 cubic meters per minute to carbonization reactor earlier is the 0.12MPa kiln gas, pumps into Ca (OH) with 40 cubic metres of/hour flows to carbonization reactor then
2Slurries, the Ca that pumps into (OH)
2Slurries are moving at illustrated bubbling carbonizing laminar flow, in the flow process with the kiln gas generation carburizing reagent of sending by the kiln gas distribution piping, overflow to down one deck column plate from sieve plate or sieve plate top after flowing to the other end, continue and kiln gas generation carburizing reagent from sieve plate top equidirectional inflow column plate layer, go out from the carbonation reaction tower tower bottom flow at last, obtaining pH value in the carbonation reaction tower outlet is 7～8, and particle diameter is the calcium carbonate serosity of 1000 nanometers, narrowly distributing, good dispersity.
Claims (5)
1. the carbonizer of a continuous synthetic calcium carbonate comprises this carbonizer jar shape body (1), and described body is provided with calcium hydroxide Ca (OH)
2Slurries input aperture (2), carbonic acid gas CO
2Input aperture (3) is provided with discharge port (4) in this body bottom, it is characterized in that:
Described Ca (OH)
2Slurries input aperture and CO
2The input aperture all is positioned at the top of body, is provided with the horizontal column plate (5) of outlet mutual dislocation below these two input apertures of body interior equably to the bottom.
2. the carbonizer of continuous synthetic calcium carbonate according to claim 1 is characterized in that: locate to be provided with the sieve plate (53) perpendicular with the first layer column plate in the outlet (52) of described the first layer column plate (51); Described CO
2The input aperture is array architecture in body so that CO
2Be covered with equably in the cavity volume of body.
3. the carbonizer of continuous synthetic calcium carbonate according to claim 1 and 2, it is characterized in that: what adopt between the outlet of described adjacent tray is S shape or snakelike reverse-flow baffle layout.
4. the production method of the lime carbonate of a carbonizer that utilizes claim 1 or 2 or 3 described continuous synthetic calcium carbonates, production stage is:
(1) calcining step--calcined limestone gets unslaked lime;
(2) the unslaked lime maturation stage--unslaked lime is converted water cure, system lime white refining liquid;
(3) carburising step--the lime extract slurries are pumped into carbonization reactor carry out carburizing reagent production precipitated chalk particle, and obtain to contain the ripe slurry of precipitated chalk particle;
(4) processed--to getting filter cake after the ripe slurry dehydration after the activation;
(5) drying treatment--filter cake is carried out drying and metering packing; Wherein,
Described carburising step is:
A. refining liquid is sent into Ca (OH)
2Slurry tank, and with deployed Ca (OH)
2Refining liquid is sent into the reactor bubble level from reactor top, simultaneously carbon dioxide is imported carbonization reactor;
Described Ca (OH)
2Refining liquid is suspension, on the horizontal column plate of this suspension in reactor and carbonic acid gas equidirectional flow between column plate, flow to the outlet that is positioned at the other end by an end, suspension enters down one deck column plate from outlet, carry out the gas, liquid, solid phase reaction in the flow process and generate precipitated chalk, reacted material is that the good ripe slurries of carbonization flow out from the reactor lower part outlet;
B. collect from reactor behind the effusive material this material carried out ageing and recarbonize or directly activate after, more after filtration, be drying to obtain product.
5. the method for continuous synthetic calcium carbonate according to claim 4 is characterized in that: Ca (OH) in the described refining liquid
2Weight concentration be 5%～15%, surplus is a water, the temperature of refining liquid is 10～60 ℃; Described carbon dioxide enters carbon dioxide volumetric concentration 〉=15% of reactor through water washing cleaning, and absolute pressure is that 0.1MPa～1.0MPa reacts.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849771A (en) * | 2012-08-29 | 2013-01-02 | 池州凯尔特纳米科技有限公司 | Continuous carbonization reaction device, and method for preparing ultrafine calcium carbonate through applying it |
| CN103408053A (en) * | 2013-05-13 | 2013-11-27 | 福建省万旗非金属材料有限公司 | Carbonization device and method for production process of precipitated calcium carbonate |
| CN104016391A (en) * | 2014-04-10 | 2014-09-03 | 连州市凯恩斯纳米材料有限公司 | Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device |
| CN104609453A (en) * | 2014-11-25 | 2015-05-13 | 广西华纳新材料科技有限公司 | Preparation method for cubic precipitated calcium carbonate |
| CN107032381A (en) * | 2017-03-20 | 2017-08-11 | 连州市凯恩斯纳米材料有限公司 | A kind of stirring-type continuous carbonization device and calcium carbonate particle synthetic method |
| CN109666187A (en) * | 2019-01-17 | 2019-04-23 | 厦门工为信息技术有限公司 | A method of precipitated calcium carbonate is prepared based on calcium hydroxide |
| CN109796035A (en) * | 2019-03-01 | 2019-05-24 | 燕卓君 | A kind of preparation method of calcium carbonate superfine powder |
| CN110115971A (en) * | 2019-06-06 | 2019-08-13 | 连州市凯恩斯纳米材料有限公司 | A kind of stirring-type continuous carbonization device and its application method |
| CN112079373A (en) * | 2020-09-10 | 2020-12-15 | 浙江浙能嘉华发电有限公司 | Device and process for preparing micron-sized homogeneous calcium carbonate through causticization reaction |
| US11377363B2 (en) | 2020-06-30 | 2022-07-05 | Arelac, Inc. | Methods and systems for forming vaterite from calcined limestone using electric kiln |
| US11577965B2 (en) | 2020-02-25 | 2023-02-14 | Arelac, Inc. | Methods and systems for treatment of lime to form vaterite |
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| US9902652B2 (en) | 2014-04-23 | 2018-02-27 | Calera Corporation | Methods and systems for utilizing carbide lime or slag |
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| CN101880051A (en) * | 2009-05-07 | 2010-11-10 | 河南科力新材料股份有限公司 | Preparation method of suspended nano-calcium carbonate for food |
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| CN1109024A (en) * | 1994-03-19 | 1995-09-27 | 颜寿地 | Method and apparatus for producing lightweight calcium carbonate |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849771A (en) * | 2012-08-29 | 2013-01-02 | 池州凯尔特纳米科技有限公司 | Continuous carbonization reaction device, and method for preparing ultrafine calcium carbonate through applying it |
| CN103408053A (en) * | 2013-05-13 | 2013-11-27 | 福建省万旗非金属材料有限公司 | Carbonization device and method for production process of precipitated calcium carbonate |
| CN104016391A (en) * | 2014-04-10 | 2014-09-03 | 连州市凯恩斯纳米材料有限公司 | Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device |
| CN104609453A (en) * | 2014-11-25 | 2015-05-13 | 广西华纳新材料科技有限公司 | Preparation method for cubic precipitated calcium carbonate |
| CN107032381B (en) * | 2017-03-20 | 2019-06-25 | 连州市凯恩斯纳米材料有限公司 | A kind of stirring-type continuous carbonization device and calcium carbonate particle synthetic method |
| CN107032381A (en) * | 2017-03-20 | 2017-08-11 | 连州市凯恩斯纳米材料有限公司 | A kind of stirring-type continuous carbonization device and calcium carbonate particle synthetic method |
| CN109666187A (en) * | 2019-01-17 | 2019-04-23 | 厦门工为信息技术有限公司 | A method of precipitated calcium carbonate is prepared based on calcium hydroxide |
| CN109796035A (en) * | 2019-03-01 | 2019-05-24 | 燕卓君 | A kind of preparation method of calcium carbonate superfine powder |
| CN109796035B (en) * | 2019-03-01 | 2021-04-23 | 湖南金箭新材料科技有限公司 | Preparation method of superfine calcium carbonate |
| CN110115971A (en) * | 2019-06-06 | 2019-08-13 | 连州市凯恩斯纳米材料有限公司 | A kind of stirring-type continuous carbonization device and its application method |
| US11577965B2 (en) | 2020-02-25 | 2023-02-14 | Arelac, Inc. | Methods and systems for treatment of lime to form vaterite |
| US11377363B2 (en) | 2020-06-30 | 2022-07-05 | Arelac, Inc. | Methods and systems for forming vaterite from calcined limestone using electric kiln |
| CN112079373A (en) * | 2020-09-10 | 2020-12-15 | 浙江浙能嘉华发电有限公司 | Device and process for preparing micron-sized homogeneous calcium carbonate through causticization reaction |
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